CN1196279A - Flotation agent for titanium fine mine and its oxidation mine - Google Patents

Abstract

A floating agent for chemical floatation of titanium ore concentrate and its oxide ore is synthetic aliphatic salt and aliphatic amine, which are prepared with new process based on existing synthesis process of fatty acid. Its advantages are high selectivity, low cost of production and no environmental pollution.

Description

Ilmenite concentrate and oxide ore flotation agent thereof

The present invention is a kind of mining flotation agent, used flotation agent when specially referring to a kind of ilmenite concentrate and oxide ore ore dressing thereof.

According to domestic existing ore-dressing technique, ore beneficiation adopted multiple scheme for example machinery, electromagnetic method and the chemistry method.Sefstromite as the Sichuan Panzhihua Iron is produced has adopted heavy electric separation when ore in sand form is selected.But heavy electric separation technology can only sort the ilmenite concentrate of particle diameter greater than 0.04mm.Particle diameter can not sort out less than this technology of 0.04mm, can only be discharged into the tailingspile.And heavy electric separation technology can only sort 15～20% ilmenite concentrate from vanadium titano-magnetite, and 80～85% ilmenite concentrate is ranked mining site with mine tailing.Make preciousness and be worth high titanium resource slatterning in vain.For a long time, the rate of sorting that how to improve ilmenite concentrate is an exploitation Panzhihua vanadium ferrotianium resource difficult problem anxious to be solved.

During with the chemical method ore dressing, the flotation agent when people have used various surfactants as ore dressing, some of them are to make with synthetic soap.Synthetic fatty acid is normally made with paraffin oxidation style.This technology is the research and development of China nearly more than 20 year, but is not very ripe, and also having much needs to improve and further perfect places.In general, its performance of the product of different process routes is different, therefore, improves existing technology, and the process of seeking the flotation agent of described ilmenite concentrate of a kind of suitable production and oxide ore thereof is that producer is pursued.

The flotation agent that the purpose of this invention is to provide a kind of ilmenite concentrate and oxide ore mine tailing thereof.This flotation agent is synthctic fat hydrochlorate and the fatty amine that adopts new special technology to produce on the basis of existing at home synthetic fatty acid technology, is used for the chemical flotation of ilmenite concentrate, has the rate of sorting height, and production cost is low, does not have environmental pollution.

For achieving the above object, the solution of the present invention is: a kind of flotation agent that is used for ilmenite concentrate and oxide ore mine tailing thereof, and its production technology comprises:

1, paraffin purifies

In reactor wax is heated to 50-70 ℃, adding acid, to adjust pH value be 2-3, add clay-filtered, pressure filtration.

2, oxidation

A, high-temperature oxydation: in special-purpose oxidizing tower, wax is warming up to 150 °-170 ℃, adds catalyst potassium permanganate or manganese ore powder (MnO ₂Content is greater than more than 60%), consumption is the heavy 0.2-0.4% of blended wax, aerating oxygen, oxidization time are about 2 hours;

B, low-temperature oxidation: will reduce to 95 °-105 ℃ through the wax liquid of high-temperature oxydation, and continue aerating oxygen, oxidization time is 14-16 hour,

3, washing

Weight ratio by oxidized petroleum waves and water is 1: 0.2-0.3 feeding temperature is 80 °-90 ° a hot water, and the impurity in the oxidizing process is removed, and number of times is at least 2 times,

4, saponification

A. in soap pan, add oxidized petroleum waves and suitable quantity of water, and be warming up to 90 °-110 ℃, add soda ash or caustic soda, add the 25-40% that alkali number is a wax liquid weight; Be made into 30% solution and add, reaction time 3-4 hour, after the reaction pH value is transferred to about 7.5, squeeze into the pressure saponification pot, pressure is added to 2-5Kg, be about 1 hour pressing time;

B. the saponification liquor later that will pressurize is squeezed into the normal pressure soap pan, is incubated 3-4 hour, again pH value is transferred to 8-8.5;

C. separate

Aliphatic acid and unsaponifiable matter are separated, promptly got described mining flotation agent.

Below in conjunction with embodiment the solution of the present invention is described in more detail.

For producing the flotation agent that is specifically designed to ilmenite concentrate and oxide ore mine tailing thereof, this process route first step is selected suitable wax stock for use, and the wax of this explained hereafter selects for use the wax of local oil plant production to produce the raw material of flotation agent.The fusing point of described wax is 42 °-50.5 ℃, and oil content is below 8%.The amount that present embodiment is produced is relevant with the volume of reactor, uses one ton of wax at every turn, and is undertaken by the process route of defined in the scheme.

One, purifies

Because contain various impurity in the paraffin raw material, for example various colloids, retinasphal etc. at first must purify.With heating paraffin fusing, fusing back wax liquid temperature is no more than 70 ℃, adds acid then in reactor, and adding sulfuric acid usually, to adjust pH value be 2-3, add clay-filtered so that adsorb described various impurity, the wax liquid that is purified of pressure filtration then,

Two, oxidation

The required equipment of oxidizing process is oxidizing tower, and this is one and has the stainless steel body of the tower, in the bubbler of stainless steel control is arranged, heating tube, cooling tube etc., and be furnished with air compressor etc.

To be added in the container of special-purpose oxidizing tower through the wax that purifies, heat hot excitation temperature to 150 °-170 ℃ of beginning aerating oxygens, and adding catalyst potassium permanganate, add the amount of about 3-5Kg in one ton of paraffin liquid, oxidation reaction is exothermic reaction, and the reaction time is about 2 hours, subsequently wax liquid temperature is reduced to and carry out the low-temperature oxidation reaction between 95 °-105 ℃, continue aerating oxygen, time 14-16 hour, become oxidized paraffin wax.The made flotation agent of this technical process is carbon containing 10-20, i.e. C10-C20, and optimum carbon chain lengths is 15, i.e. C15, this molecular structure is best as the effect of flotation agent.

Oxidized paraffin wax after peroxidating will remove low molecular acid and catalyst residue etc. through washing, because these two kinds of materials are all water-soluble, and wax and water are immiscible.Washing temperature is between 80 °-90 ℃, and washing times is three times.

Three, saponification

In soap pan, add oxidized petroleum waves and water, be warming up to 90 °-110 °, add soda ash 40Kg, it is mixed with alkalinity is 30% aqueous slkali 200Kg, slowly adds, and starts agitating device, reaction time 3-4 hour, after the reaction pH value is transferred to about 7.5, squeeze into the pressure saponification pot, open steam pressurized.Pressure is added to 3Kg, keep about 1 hour.

Saponification liquor behind the compressive reaction is squeezed into the normal pressure soap pan, be incubated 3 hours, transfer about pH value to 8 again.

Contain 40% the water of having an appointment in the above-mentioned saponification liquor, soap and unsaponifiable matter etc. utilize in the water dissolution characteristics that it is separated, and promptly obtain described flotation agent.

The mining processing industry that the flotation agent product that obtains is used for ilmenite concentrate and oxide ore thereof is tested, and has satisfied the titanium dioxide (TiO of ilmenite concentrate ₂) grade reaches more than 47%, yield reaches 60% designing requirement, and free from environmental pollution, and the water of discharging after ore dressing no longer turns black, and discharging meets requirement on environmental protection.Applying unit has obtained huge economic benefit and social benefit.

In sum, the present invention is effective.

Claims (1)

1, a kind of flotation agent that is used for ilmenite concentrate and oxide ore thereof is characterized in that:

1. paraffin purifies

In reactor wax is heated to 50-70 ℃, adding acid, to adjust pH value be 2-3, adds clay-filtered, the press filtration separation,

2. oxidation

A. high-temperature oxydation: in special-purpose oxidizing tower, wax is warming up to 150 °-170 ℃, adds catalyst potassium permanganate or manganese ore powder (MnO ₂Content is greater than on 60%), consumption is the heavy 0.2-0.4% of blended wax, aerating oxygen, oxidization time are about 2 hours.

B, low-temperature oxidation: will reduce to 95 °-105 ℃ through the wax liquid of high-temperature oxydation, and continue aerating oxygen, oxidization time is 14-16 hour,

3., washing

Weight ratio by oxidized petroleum waves and water is 1: 0.2-0.3 feeding temperature is 80 °-90 ° a hot water, and the impurity in the oxidizing process is removed, and number of times is at least secondary,

4., saponification

A. in soap pan, add oxidized petroleum waves and suitable quantity of water, and be warming up to 90 °-110 ℃, add soda ash or caustic soda, add the 25-40% that alkali number is a wax liquid weight, be made into 30% solution adding, reaction time 3-4 hour, after the reaction PH is transferred to about 7.5, squeezes into the pressure saponification pot, pressure is added to 2-5Kg, be about 1 hour pressing time

B, the saponification liquor later that will pressurize are squeezed into the normal pressure soap pan, are incubated 3-4 hour, again pH value are transferred to 8-8.5.

C, separation

Aliphatic acid and unsaponifiable matter are separated, promptly got described mining flotation agent.